反应 #2507833

ord-0a742841cf404074ab18670d412b94fc

反应方程式

CCCCCC1COc2cc(C=CC3=Cc4cc(F)cc(F)c4OC3)c(F)cc2C1
6,8-Difluoro-3-[2-(6-fluoro-3-pentylchroman-7-yl)vinyl]-2H-chromene
CCCCCC1COc2cc(CCC3=Cc4cc(F)cc(F)c4OC3)c(F)cc2C1
6,8-Difluoro-3-[2-(6-fluoro-3-pentylchroman-7-yl)ethyl]-2H-chromene

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The catalyst is filtered off
  2. 2
    其他the solution is evaporated
  3. 3
    过滤the residue is filtered through silica gel with toluene/heptane (3:2)
  4. 4
    其他the crude product is recrystallised from n-heptane at −25° C.
  5. 5
    其他giving colourless crystals of m.p. 84° C.

实验过程

6,8-Difluoro-3-[2-(6-fluoro-3-pentylchroman-7-yl)vinyl]-2H-chromene is dissolved in THF and hydrogenated to completion on a palladium/active carbon catalyst. The catalyst is filtered off, the solution is evaporated, the residue is filtered through silica gel with toluene/heptane (3:2), and the crude product is recrystallised from n-heptane at −25° C., giving colourless crystals of m.p. 84° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07955664B2uspto-grants-2011_06